ES2565502T3 - Métodos de recubrimiento de una lata de comida o bebida - Google Patents
Métodos de recubrimiento de una lata de comida o bebida Download PDFInfo
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- ES2565502T3 ES2565502T3 ES11169890.8T ES11169890T ES2565502T3 ES 2565502 T3 ES2565502 T3 ES 2565502T3 ES 11169890 T ES11169890 T ES 11169890T ES 2565502 T3 ES2565502 T3 ES 2565502T3
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- B65D17/00—Rigid or semi-rigid containers specially constructed to be opened by cutting or piercing, or by tearing of frangible members or portions
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- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
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- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/13—Hollow or container type article [e.g., tube, vase, etc.]
- Y10T428/1352—Polymer or resin containing [i.e., natural or synthetic]
- Y10T428/139—Open-ended, self-supporting conduit, cylinder, or tube-type article
- Y10T428/1393—Multilayer [continuous layer]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
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- Y10T428/31681—Next to polyester, polyamide or polyimide [e.g., alkyd, glue, or nylon, etc.]
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- Y10T428/31688—Next to aldehyde or ketone condensation product
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/31696—Including polyene monomers [e.g., butadiene, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/31699—Ester, halide or nitrile of addition polymer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
Un método de recubrimiento de una lata de comida o bebida, comprendiendo el método: proporcionar una composición de recubrimiento que comprende un polímero de látex polimerizado por emulsión, en la que el polímero de látex polimerizado por emulsión: (i) comprende un producto de reacción de un componente de monómero etilénicamente insaturado polimerizado en presencia de una dispersión acuosa de una sal de polímero, en el que el componente de monómero etilénicamente insaturado incluye al menos un monómero que contiene un grupo funcional oxirano, y (ii) está sustancialmente libre de bisfenol A de enlace y compuestos de glicidil éter aromático; y aplicar la composición de recubrimiento a un sustrato de metal antes o después de formar el sustrato de metal en una lata de comida o bebida o una porción de la misma.
Description
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divalente, preferentemente ciclohexileno. Se contempla que Y pueda ser tan grande como se desee para la aplicación particular, que un experto en la materia puede determinar fácilmente.
Preferentemente, Y proporciona estabilidad hidrolítica a al menos uno de los enlaces éster adyacentes a R1 en la Fórmula I. Esto puede conseguirse mediante la selección de Y que incluye un grupo estéricamente voluminoso que está en la proximidad (preferentemente dentro de dos átomos) de al menos uno de los átomos de oxígeno del éster en la Fórmula I.
En ciertas realizaciones, R1 tiene la fórmula -(C(R2)2)s- en la que s es al menos 2, y preferentemente, s es al menos 3, en la que cada R2 es como se ha definido anteriormente. Ejemplos de dichos grupos R1 incluyen, por ejemplo, neopentileno, butiletilpropileno y -CH2-CH(CH3)-CH2-.
En ciertas realizaciones, Y tiene la fórmula
-[Zw-C(R2)2-O-C(O)-R3-C(O)-O-C(R2)2-]vZw-,
en la que w es 0 o 1, v es de 1 a 10, cada R2 es como se ha definido anteriormente, cada R3 es independientemente un grupo orgánico divalente, y cada Z es independientemente un grupo orgánico divalente.
En ciertas realizaciones, R3 es un grupo alifático saturado divalente (es decir, grupo alquileno ramificado o no ramificado), un grupo alicíclico divalente, un grupo arileno, o combinaciones de los mismos. En ciertas realizaciones, R3 es un grupo alquileno(C3-C20) (ramificado o no ramificado) o un grupo fenileno.
En ciertas realizaciones, Z es un grupo alifático saturado divalente (es decir, grupo alquileno ramificado o no ramificado), un grupo alicíclico divalente, un grupo aromático divalente (es decir, un grupo arileno), o combinaciones de los mismos.
Preferentemente, Z proporciona estabilidad hidrolítica a al menos uno de los enlaces de éster adyacentes a R1 en la Fórmula I y/o a un enlace de éster adyacente contenido dentro de Y. Esto puede conseguirse por la selección de Z que incluye un grupo estéricamente voluminoso que está en la proximidad (preferentemente en el rango de dos átomos de distancia) de al menos uno de los átomos de oxígeno del éster.
En los segmentos de Fórmula I, n es preferentemente 0 (es decir, R no está presente). Si n es 1 y R está presente, sin embargo, es preferentemente un grupo alquileno(C1-C4), y más preferentemente un resto alquileno(C1-C4).
En los segmentos de Fórmula I, cada Ar tiene preferentemente menos de 20 átomos de carbono, más preferentemente menos de 11 átomos de carbono, e incluso más preferentemente menos de 8 átomos de carbono. Preferentemente, Ar tiene al menos 4 átomos de carbono, más preferentemente al menos 5 átomos de carbono, e incluso más preferentemente, al menos 6 átomos de carbono.
En ciertas realizaciones, cada Ar es un grupo fenileno. En ciertas realizaciones, cada Ar es un grupo fenileno de la fórmula -C6(R4)4-, en la que cada R4 es independientemente hidrógeno, un halógeno, o un grupo orgánico, y en la que dos grupos R4 pueden unirse para formar un anillo que contiene opcionalmente uno o más heteroátomos. En ciertas realizaciones, R4 es hidrógeno o un grupo orgánico, en las que dos grupos R4 pueden unirse para formar un anillo de 6 miembros. Preferentemente, R4 es hidrógeno.
Pueden prepararse polímeros de poliéster tales como estos mediante una variedad de métodos a partir de los compuestos de Fórmula II:
HO-Ar-Rn-C(O)-O-R1-O-C(O)-Rn-Ar-OH
en la que Ar, R, R1 y n son como se ha definido anteriormente. Dichos compuestos pueden prepararse, por ejemplo, mediante la reacción de esterificación de un mol de un diol (por ejemplo, HO-R1-OH tales como, por ejemplo, 1,4ciclohexano dimetanol, neopentilglicol, 2-butil-2-etil-1,3-propano diol, o 2-metil-1,3-propano diol) con dos moles de un ácido (por ejemplo, ácido 4-hidroxi benzoico). Como alternativa, dichos compuestos pueden prepararse, por ejemplo, mediante la reacción de transesterificación de un mol de un diol (por ejemplo, 1,4-ciclohexano dimetanol, neopentil glicol, 2-butil-2-etil-1,3-propano diol, o 2-metil-1,3-propano diol) con dos moles de un éster (por ejemplo, 4-hidroxi metil benzoato, 4-hidroxi etil benzoato, o 4-hidroxi butil benzoato).
Pueden prepararse polímeros de Fórmula I mediante métodos que implican desarrollar el peso molecular de los compuestos de Fórmula II. En ciertas realizaciones, los compuestos de Fórmula II (por ejemplo, fenoles dihídricos) pueden hacerse reaccionar con un diepóxido para desarrollar el peso molecular. Por ejemplo, compuestos de Fórmula II (por ejemplo, fenoles dihídricos) pueden hacerse reaccionar en gran medida con diepóxidos no basados en BPA y BPF de la misma manera que el Bisfenol A o Bisfenol F lo hace, para generar polímeros que pueden formularse con reticulantes y aditivos para recubrimientos para envasado rígido. Por ejemplo, los compuestos de Fórmula II pueden hacerse reaccionar con un diepóxido para formar un polímero que incluya segmentos -CH2
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soldada, cada lata requiere típicamente una capa de recubrimiento líquido, que protege la "soldadura" expuesta de la corrosión posterior u otros efectos al producto alimenticio contenido. Los recubrimientos líquidos que tienen este papel se denominan "tiras de costura lateral". Las tiras de costura lateral típicas se aplican por pulverización y se curan rápidamente con el calor residual de la operación de soldadura además de un horno térmico, ultravioleta, y/o electromagnético pequeño.
Otras aplicaciones comerciales del recubrimiento y métodos de curado también contemplan, por ejemplo, electrorrecubrimiento, recubrimiento por extrusión, laminado, recubrimiento en polvo, y similares.
Los recubrimientos preferidos de la presente invención muestran una o más de las propiedades que se han descrito en la Sección de Ejemplos. Los recubrimientos más preferidos de la presente invención muestran una o más de las siguientes propiedades: valor de exposición de metal de menos de 3 mA; valor de exposición de metal después del daño por caída de menos de 3,5 mA; resultados de extracción global de menos de 50 ppm; proporción de adhesión de 20; proporción de alteración superficial del color de al menos 7; agrietamiento leve o ausencia en un ensayo de impacto inverso; sin agrietamiento (proporción de 10) en un ensayo de impacto domo; biselado por debajo de 0,51 cm (0,2 pulgadas); intervalo COF de 0,055 a 0,095; y después de la pasteurización o esterilización en retorta, una continuidad de menos de 20 mA.
A continuación, se resumen las realizaciones divulgadas en la presente solicitud:
1. Un método de recubrimiento de una lata de comida o bebida, el método comprende:
formar una composición que comprende un polímero de látex polimerizado por emulsión, que comprende:
formar una sal de un polímero ácido- o anhídrido-funcional y una amina en un transportador que comprende agua para formar una dispersión acuosa; combinar un componente de monómero etilénicamente insaturado con la dispersión acuosa; y polimerizar el componente de monómero etilénicamente insaturado en presencia de la dispersión acuosa para formar un polímero de látex polimerizado por emulsión; y
aplicar la composición que comprende el polímero de látex polimerizado por emulsión a un sustrato de metal antes de o después de conformar el sustrato de metal en una lata de comida o bebida o parte de la misma.
- 2.
- El método del punto 1, en el que la aplicación de la composición a un sustrato de metal comprende aplicar la composición al sustrato de metal en forma de una bobina o lámina plana, endurecer el polímero de látex polimerizado por emulsión, y formar el sustrato en una lata de comida o bebida o parte de la misma.
- 3.
- El método del punto 2, en el que conformar el sustrato en una lata o parte de la misma comprende conformar el sustrato en una tapa de lata o un cuerpo de lata.
- 4.
- El método del punto 2, en el que la lata es una lata de comida embutida de 2 piezas, lata de comida de 3 piezas, tapa de lata de comida, lata embutida y planchada, tapa de lata de bebida, y similares.
- 5.
- El método del punto 1, en el que el sustrato de metal comprende acero o aluminio.
- 6.
- El método del punto 1, en el que la aplicación de la composición a un sustrato de metal comprende la aplicación de la composición al sustrato de metal después de que el sustrato de metal se forme en una lata o parte de la misma.
- 7.
- El método del punto 1, en el que la combinación de un componente de monómero etilénicamente insaturado con la dispersión acuosa comprende añadir el componente de monómero etilénicamente insaturado a la dispersión acuosa.
- 8.
- El método del punto 7, en el que el componente de monómero etilénicamente insaturado se añade progresivamente a la dispersión acuosa.
- 9.
- El método del punto 1, en el que el componente de monómero etilénicamente insaturado comprende una mezcla de monómeros.
- 10.
- El método del punto 9, en el que la mezcla de monómeros comprende al menos un monómero que contiene un grupo funcional oxirano.
- 11.
- El método del punto 10, en el que la mezcla de monómeros comprende al menos un monómero alfa, betaetilénicamente insaturado que contiene un grupo funcional oxirano.
- 12.
- El método del punto 10, en el que el monómero que contiene un grupo funcional oxirano está presente en el
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en miliamperios. Típicamente, se someten inicialmente a ensayo las continuidades de la tapa y después, las tapas se someten a pasteurización o esterilización en retorta.
Los recubrimientos preferidos de la presente invención pasan inicialmente menos de 10 miliamperios (mA) cuando
5 se someten a ensayo como se ha descrito anteriormente, más preferentemente menos de 5 mA, lo más preferible menos de 2 mA, y de forma óptima menos de 1 mA. Después de la pasteurización o esterilización en retorta, los recubrimientos preferidos proporcionan continuidades de menos de 20 mA, más preferentemente menos de 10 mA, incluso más preferentemente menos de 5 mA, e incluso más preferentemente menos de 2 mA.
10 Lista de Materias Primas e Ingredientes
La siguiente tabla enumera algunas de las materias primas e ingredientes usados en los siguientes ejemplos. Como apreciará el experto en la materia, pueden sustituirse por materiales o proveedores alternativos
- Nombre Químico
- Nombre Comercial Proveedor Ubicación
- Ácido Metacrílico Glacial
- Rohm & Haas Philadelphia, PA
- Butil Acrilato
- Rohm & Haas Philadelphia, PA
- Estireno
- Rohm & Haas Philadelphia, PA
- Peróxido de Benzoílo
- Norac Company Helena, AR
- Butanol
- Dow Midland, MI
- Butil éter de Etilenglicol
- Butyl Cellosolve/Dowanol EB Dow Midland, MI
- Butil Metacrilato
- Rohm & Haas Philadelphia, PA
- Peroctoato de t-Butilo
- Arkema Philadelphia, PA
- Etil acrilato
- Rohm & Haas Philadelphia, PA
- Ácido acrílico
- Rohm & Haas Philadelphia, PA
- Hidroxipropilmetacrilato
- ROCRYL 410 Rohm & Haas Philadelphia, PA
- Hidroxietil metacrilato
- ROCRYL 400 Rohm & Haas Philadelphia, PA
- Dimetiletanol amina
- Huntsman Chemical Dallas, TX
- Glicidil metacrilato
- SR 379 Sartomer, Inc Warrington, PA
- Peróxido de Hidrógeno
- Ashland Chemical Pittsburgh, PA
- Benzoína
- Estron Calvert City, KY
- N-Isobutoximetacrilamida
- Monómero CYLINK IBMA Cytec Ind. West Patterson, NJ
- Alcohol amílico
- Dow Midland, MI
- Butil éter de Propilenglicol
- DOWANOL PNB Dow Midland, MI
- Alcohol etoxilado secundario
- TERGITOL 15-S-7 Dow Midland, MI
- sec-butanol
- Dow Midland, MI
- Cera de Polietileno
- Slipayd 404 Elementis Staines, UK
- Fenólico basado en Fenol Termoestable
- SD-912B Valspar Minneapolis, MN
- Emulsión de cera de Carnuba
- Michemlube 160 PFE Michelman Cincinnati, OH
- Alcohol isooctílico
- Aldrich Chemical Milwaukee, WI
- Cera de Polietileno
- Lanco Glidd 5118 Lubrizol Wickliffe, OH
- Dipropilenglicol
- Aldrich Chemical Milwaukee, WI
- Ácido Isoftálico
- BP Amoco Chicago, IL
- Óxido de Dibutil estaño
- Fastcat 4201 Arkema Philadelphia, PA
- Xileno
- Exxon Newark, NJ
- Anhídrido Trimelítico
- BP Amoco Chicago, IL
- Complejo de Hierro
- Hamp-OL 4,5 % Iron Traylor Chemical Orlando, FL
- Ácido eritórbico
- Aldrich Chemical Milwaukee, WI
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- Nombre Químico
- Nombre Comercial Proveedor Ubicación
- T-Butilhidoperóxido
- Trigonox A-W70 Akzo Philadelphia, PA
- Etilenglicol
- Ashland Chemical Pittsburgh, PA
- Ácido sebácico
- Ivanhoe Indutries Tampa. FL
- 1,4-ciclohexano dimetanol al 90 % en agua
- CHDM-90 Eastman Kingsport, TN
- Ácido Buti Estanoico
- Fastcat 4100 Arkema Philadelphia, PA
- Ácido 4-Hidroxibenzoico
- Acros Organics through Fisher Scientific Houston, TX
- Diglicidil éter de 1,4ciclohexano dimetanol
- Erisys GE-22 CVC Specialty Chemicals Maple Shade, NJ
- Yoduro de etiltrifenil fosfonio
- Catalyst 1201 Deepwater Chemicals Woodward, OK
- Anhídrido succínico
- JLM Marketing Tampa, FL
- Bisfenol A
- Dow Midland, MI
- Diglicidil éter de Bispenol A
- Epon 828 Resolution Performance Products Houston, TX
- Metilisobutil cetona
- Dow Midland, MI
- Éster dibásico
- Dupont Wilminton, DE
- Metil éter de propilenglicol
- Dowanol PM Dow Midland, MI
Ejemplo de Referencia 1: Realización 1. Preparación de Acrílico Ácido-Funcional
Se preparó una premezcla de 512,6 partes de ácido metacrílico glacial (MAA), 512,6 partes de acrilato de butilo (BA), 114,0 partes de estireno, y 73,2 partes de peróxido de benzoílo (humedad al 70 %) en un recipiente separado. Se equipó un matraz de 3 litros con un agitador, condensador de reflujo, termopar, manta calefactora, y una atmósfera protectora de nitrógeno. Se añadió el diez por ciento de la premezcla al matraz junto con 405,9 partes de butanol y 30,6 partes de agua desionizada. A la premezcla restante se añadieron 496,1 partes de butanol y 38,3 partes de agua desionizada. Con la atmósfera protectora de nitrógeno fluyendo en el matraz, los contenidos se calentaron a 93 ºC. A 93 ºC, el calentamiento externo se detuvo y se dejó que el material aumentase su temperatura durante quince minutos. Después de quince minutos, el lote estaba a 97 ºC, y la premezcla restante se añadió uniformemente durante dos horas manteniendo de 97 ºC a 100 ºC. Cuando la adición de premezcla se completó, el recipiente de premezcla se aclaró con 5 partes de butanol. El lote se mantuvo a la misma temperatura durante dos horas y media. El calentamiento fue discontinuo y se añadieron 317,7 partes de butil cellosolve. El prepolímero acrílico resultante tuvo sólidos (NV) al 44,3 %, con un índice de acidez de 313 y una viscosidad Brookfield (según se determina por la norma ASTM D-2196) de 4.990 centipoise (cps).
Ejemplo de Referencia 1: Realización 2. Preparación de Acrílico Ácido-Funcional
Se preparó una premezcla de 677,7 partes de ácido metacrílico glacial, 677,7 partes de metacrilato de butilo (BMA), 150,8 partes de estireno, y 96,9 partes de peróxido de benzoilo (humedad al 70 %) se preparó en un recipiente separado. Se equipó un matraz de 5 litros con un agitador, condensador de reflujo, termopar, manta calefactora, y una atmósfera protectora de nitrógeno. Se añadió el diez por ciento de la premezcla al matraz junto con 536,9 partes de butanol y 40,7 partes de agua desionizada. A la premezcla restante se añadieron 758,1 partes de butanol y 50,6 partes de agua desionizada. Con la atmósfera protectora de nitrógeno fluyendo en el matraz, los contenidos se calentaron a 93 ºC. A 93 ºC, el calentamiento externo se detuvo y se dejó que el material aumentase su temperatura durante diez minutos. Después de diez minutos, el lote estaba a 98 ºC, y la premezcla restante se añadió uniformemente durante dos horas manteniendo de 97 ºC a 100 ºC. El lote se mantuvo a la misma temperatura durante tres horas. El calentamiento fue discontinuo y el lote se enfrió. El prepolímero acrílico resultante tuvo NV al 49,9 %, con un índice de acidez de 304 y una viscosidad Brookfield de 101.000 centipoise.
Ejemplo de Referencia 1: Realización 3. Preparación de Acrílico Ácido-Funcional
Se preparó una premezcla de 802,6 partes de ácido metacrílico glacial, 807 partes de metacrilato de butilo, 178,5 partes de estireno, 80,3 partes de peroctoato de t-butilo, 838,5 partes de butanol y 59,9 partes de agua desionizada en un recipiente separado. Se equipó un matraz de 5 litros con un agitador, condensador de reflujo, termopar, manta calefactora, y una atmósfera protectora de nitrógeno. Se añadieron al matraz de 5 litros 635,8 partes de butanol y 48,1 partes de agua desionizada. El matraz se calentó a 94 ºC. A 94 ºC, se añadieron 12,5 partes de peroctoato de t-butilo. El lote se mantuvo durante cinco minutos después de lo cual la premezcla se añadió durante dos horas y
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Tabla 5: Experimento de Diseño de Emulsión
- Ejemplo 3:
- Realización 11 Realización 12 Realización 13 Realización 14 Realización 15 Realización 16 Realización 17 Realización 18
- Proporción Acrílico/ Monómero
- 73/27 65/35
- Composición de Monómero 1
- Composición de Monómero 2 Composición de Monómero 1 Composición de Monómero 2
- Nivel GMA
- Bajo Alto Bajo Alto Bajo Alto Bajo Alto
- Monómeros
- Estireno
- 42 39 33 33 43 41 33 33
- BA
- 54 53 40 41 54 53 40 40
- BMA
- 0 0 23 18 0 0 24 21
- GMA
- 4 8 4 8 3 6 3 6
- 32,0 %l
- 31,3 % 31,6 % 31,9 % 31,6 % 32,0 % 31,7 % 32,0 %
- Viscosidad (Copa Ford n.º 4)
- -- 63 s -- -- 35 s 210 s 42 s ---
- Viscosidad Brookfield (cps)
- 10.000 -- 10.000 695 -- -- -- 1.384
- Índice de acidez
- 74,7 72,9 74,9 70,2 101 96,1 101 96,5
Se sometieron a ensayo las estructuras reticulares de la Tabla 5 sin modificación o formulación adicional, y los resultados se muestran en la Tabla 6. Cada composición se depositó sobre aluminio Alcoa ALX con un peso de película de 1,1-1,25 miligramos por centímetro cuadrado (mg/cm2) (7-8 miligramos por pulgada cuadrada (msi)) y se curó durante 10 segundos para conseguir un pico de temperatura de metal de 215 ºC (420°F) en un horno de bobina alimentado por gas.
Tabla 6: Rendimiento de Película de Tapa de Bebida
- Control basado en agua1
- Ej. 3: Realización 11 Ej. 3: Realización 12 Ej. 3: Realización 13 Ej. 3: Realización 14 Ej. 3: Realización 15 Ej. 3: Realización 16 Ej. 3: Realización 17 Ej. 3: Realización 18
- Agrietamiento
- Ninguno Ninguno Ninguno Ninguno Ninguno Ninguno Leve Ninguno Ninguno
- Resistencia MEK
- 19 5 6 3 7 5 6 4 8
- Biselado4
- 0,343 0,013 0,020 0,071 0,003 0,020 0,013 0,030 0,013
- Retorta de Agua2
- Alteración superficial del color
- 9,5 10 9,5 9,5 9,5 9 10 8 10
- Adhesión
- 10 10 10 10 10 10 10 10 10
- Pasteurizaión3
- Alteración superficial del color
- 10 10 10 10 10 10 10 10 10
- Adhesión
- 10 10 10 10 10 10 10 10 10
- Continuidad de la Tapa
- Inicial
- 0 0,22 25,3 11,5 57,8 17,7 133,5 27,5 132,2
- Después de Retorta2
- 8,4 31,8 No Sometido a Ensayo 31,7 No Sometido a Ensayo No Sometido a Ensayo No Sometido a Ensayo 34,3 No Sometido a Ensayo
- 1 Recubrimiento de tapa de bebida disponible comercialmente de Valspar código 13Q80AG. 2 90 minutos a 121 ºC (250 ºF). 3 30 minutos a 85 ºC (185 ºF). 4 Realizado después de una pasteurización de 45 minutos a 85 ºC (185 ºF). Medido en centímetros.
10 Ejemplo 3: Realizaciones 5b y 19-25
Se preparó un diseño de experimento según el Ejemplo 2: La realización 4, como sal acrílica de ácido funcional y el proceso que se ha indicado anteriormente se describe en la Tabla 7. El Ejemplo 3: Realización 5b, se incluyó como 15 una de las variables y fue una repetición de la Realización 5.
26
Tabla 7: Experimento de Diseño de Emulsión
- Ejemplo 3:
- Realización 19 Realización 20 Realización 5b Realización 21 Realización 22 Realización 23 Realización 24 Realización 25
- Proporción Acrílico/Monóm ero
- 73/27 65/35
- Composición de Monómero 1
- Composición de Monómero 2 Composición de Monómero 1 Composición de Monómero 2
- Nivel GMA
- Bajo Alto Bajo Alto Bajo Alto Bajo Alto
- Monómeros
- Estireno
- 42 39 33 33 43 41 33 33
- BA
- 54 53 40 41 54 53 40 40
- BMA
- 0 0 23 18 0 0 24 21
- GMA
- 4 8 4 8 3 6 3 6
- Sólidos
- 31,5 % 31,6 % 31,6 % 31,4 % 31,3 % 31,6 % 31,5 % 31,7 %
- Viscosidad (Copa Ford n.º 4)
- 55 s 60 s 50 s 56 s 106 s --- 70 s ---
- Viscosidad Brookfield (cps)
- --- --- --- --- --- 2.624 --- 3.000
- Índice de acidez
- 71,9 73,0 69,0 68,3 95,4 92,5 94,7 98,0
Las estructuras reticulares a partir de la Tabla 7 se cometieron a ensayo sin modificación o formulación adicional, y los resultados se muestran en la Tabla 8. Cada composición se depositó sobre aluminio Alcoa ALX con un peso de lámina de 1,1-1,25 mg/cm2 (7-8 msi) y se curó durante 10 segundos para conseguir un pico de temperatura de metal de 215 ºC (420 ºF) en un horno de bobina alimentado por gas.
Tabla 8. Rendimiento de Película de Tapa de Bebida
- Control basado en agua1
- Ej. 3: Realización 19 Ej. 3: Realización 20 Ej. 3: Realización 5b Ej. 3: Realización 21 Ej. 3: Realización 22 Ej. 3: Realización 23 Ej. 3: Realización 24 Ej. 3: Realización 25
- Agrietamiento
- Ninguno Ninguno Ninguno Ninguno Ninguno Ninguno Leve Ninguno Sí
- MEK
- 19 4 7 4 10 6 11 4 6
- Biselado4
- 0,343 0,064 0,051 0,038 0,033 0,056 0,013 0,046 0,013
- Retorta de Agua2
- Alteración superficial del color
- 9,5 9,5 9,5 10 10 9,5 10 7 9,5
- Adhesión
- 10 10 10 10 10 10 10 10 10
- Pasteurizaión3
- Alteración superficial del color
- 10 10 10 10 10 10 10 10 10
- Adhesión
- 10 10 10 10 10 10 10 10 10
- Continuidad de la Tapa
- Inicial
- 0 5,5 2,6 6,0 12,3 20,2 61,2 1,9 93,6
- Después de Retorta2
- 8,4 23,5 143 23,4 134,0 78,8 No Sometido a Ensayo 52,5 No Sometido a Ensayo
- 1 Recubrimiento de tapa de bebida disponible comercialmente de Valspar código 13Q80AG. 2 90 minutos a 121 ºC (250 ºF). 3 30 minutos a 85 ºC (185 ºF). 4 Realizado después de una pasteurización de 45 minutos a 85 ºC (185 ºF). Medido en centímetros.
10 Ejemplo 3: Realizaciones 26-33 Se preparó un diseño de experimento según el Ejemplo 2: La realización 11 como la sal acrílica de ácido funcional y el proceso que se ha indicado anteriormente se describe en la Tabla 9. 15
27
- Control basado en agua1
- Ejemplo 4: Realización 3 Ejemplo 4: Realización 4
- Impacto en Domo
- 10 10 10
- Resistencia a Isopropanol
- >100 >100 5 - 10
- Retorta de Agua2
- Alteración superficial del color
- 7 10 10
- Adhesión
- 10 10 10
- Ensayo de Detergente Joy
- Alteración superficial del color
- 7 10 10
- Adhesión
- 10 10 10
- Extracciones globales3
- <0,1 ppm4 <0,1 ppm4 <0,1 ppm4
- 1 Recubrimiento de lata de bebida interior disponible comercialmente de Valspar código 10Q45AF. 2 90 minutos a 121 ºC (250 ºF). 3 2 horas a 65,56 ºC (150 ºF) en etanol acuoso al 90 %. 4 Por debajo del límite de detección de corriente.
Como se puede ver en la Tabla 17, los recubrimientos de la presente invención se comparan de forma favorable al recubrimiento de epoxi-acrilato comercial, y existe un beneficio sustancial en la resistencia a retorta.
5 Ejemplo 5: Realización 1. Recubrimiento de Bobina de la Tapa de Bebida
Se agitaron en un tarro con un agitador, 483,25 partes de la emulsión del Ejemplo 3: Realización 5 con 16,75 partes de cera SLIPAYD 404. La mezcla se agitó durante 10 minutos para hacerla uniforme. Después, la mezcla se filtró. La mezcla tuvo aproximadamente sólidos al 31 %. La mezcla se aplicó a 7-8 miligramos por pulgada cuadrada (msi)
10 (1,1-1,25 mg/cm2) sobre aluminio ALX Alcoa y se secó en horno durante 10 segundos (s) para conseguir un pico de temperatura de metal de 204 ºC (400 ºF) en un horno de bobina. También se aplicó a 7-8 msi (1,1-1,25 mg/cm2) sobre aluminio ALX Alcoa y se secó en horno durante 10 segundos para conseguir un pico de temperatura de metal de 224 ºC (435 ºF) en un horno de bobina. Las propiedades de película se muestran en la Tabla 18.
15 Tabla 18: Propiedades de Película de Tapa de Bebida
- Control basado en agua1
- Ejemplo 5 Realización 1
- Secado en horno
- 10 s para conseguir 204 ºC (400 ºF) 10 s para conseguir 224 ºC (435 ºF) 10 s para conseguir 204 ºC (400 ºF) 10 s para conseguir 224 ºC (435 ºF)
- Res. MEK
- 23 35 4 4
- Biselado2
- 0,500 0,193 0,018 0,010
- Dowfax3
- Alteración superficial del color
- 4 9 4 9
- Adhesión
- 10 10 10 10
- Pasteurización 4
- Alteración superficial del color
- 6 9 5 10
- Adhesión
- 10 10 10 10
- Retorta de Agua5
- Alteración superficial del color
- 6,5 10 5,5 10
- Adhesión
- 10 10 10 10
- Continuidades de Tapa
- Inicial Después Inicial Después Inicial Después Inicial Después
- Pasteurización4
- 0,13 0,33 0,06 0,28 2,76 21,35 1,5 17,9
- Retorta de Agua5
- 0,016 2,22 0,06 0,52 4,16 22,9 1,4 17,55
- 1 Recubrimiento de tapa de bebida disponible comercialmente de Valspar código 13Q80AG.
33
Tabla 21: Formulación de Tapa de Bebida
- Ejemplo 5 Realización 5
- Composición
- Ejemplo 3, Realización 38
- 90,80
- Dowanol PNP 1
- 2,425
- Dowanol DPNB 1
- 2,425
- Alcohol Isooctílico
- 1,54
- Michem Lube 160 PFE
- 0,57
- Lanco Glidd 5118 2
- 2,24
- Sólidos (%)
- 27,5 - 29,5
- Viscosidad (Copa Ford n.º 4)
- 20 s - 30 s
- 1 Disponible comercialmente de Dow Chemical 2 Lubricante disponible comercialmente de Lubrizol Corp.
Tabla 22: Rendimiento de Película de la Formulación de Tapa de Bebida
- Control Basado en Agua1
- Ejemplo 5 Realización 5
- Secado en horno
- 10 s para conseguir 204 ºC (400 ºF) 10 s para conseguir 215 ºC (420 ºF) 10 s para conseguir 204 ºC (400 ºF) 10 s para conseguir 215 ºC (420 ºF)
- Res. MEK
- 34 40 10 8
- Biselado4
- 0,178 0,094 0,074 0,038
- Dureza al Lápiz
- 3H - 4H 3H HB HB
- COF
- 0,068 0,076 0,068 0,075
- Pasteurización2
- Alteración superficial del color
- 10 10 9 10
- Adhesión
- 10 10 10 10
- Retorta de Agua3
- Alteración superficial del color
- 9 10 8 9
- Adhesión
- 10 10 10 10
- Continuidades de Tapa
- Inicial Después Inicial Después Inicial Después Inicial Después
- Pasteurización2
- 0,0 0,1 1,1 17,6 0,5 0,7 0,5 4,3
- Retorta de Agua3
- 0,05 0,15 1,4 11,2 0,15 0,35 0,78 10,5
- 1 Recubrimiento de tapa de bebida disponible comercialmente de Valspar código 13Q80AG. 2 30 minutos a 85 ºC (185 ºF). 3 90 minutos a 121 ºC (250 ºF). 4 Realizado después de una pasteurización de 45 minutos a 85 ºC (185 ºF). Medido en centímetros.
5 Los resultados a partir de la Tabla 22 muestran que una formulación de tapa de bebida de la presente invención puede proporcionar un rendimiento similar a un recubrimiento de tapa de bebida acuoso basado en epoxi comercial incluso con una resistencia de disolvente menor como se mide por dobles frotamientos MEK. También hay un beneficio adicional en una mejor resistencia al biselado.
10 Ejemplo 6: Látex con Estabilizador de Poliéster
El Ejemplo 6 se diseña para ilustrar que el uso de una sal de polímero ácido-funcional diferente como estabilizador para una emulsión de la presente invención. 15 Etapa A
Se equipó un matraz de 2 litros con un agitador, columna de relleno, colector Dean Stark, condensador de reflujo, termopar, manta calefactora, y una atmósfera protectora de nitrógeno. Al matraz se añadieron 700,1 partes de
35
premezcla de monómero se aclaró con 81,6 partes de agua desionizada, que se añadió también al matraz. Los contenidos del matraz se agitaron durante 10 minutos, después de lo cual se añadió el 10 % de la tercera premezcla dentro de un minuto. Una vez que estuvo el 10 % de la tercera premezcla, la temperatura se aumentó a 37 ºC y el lote se mantuvo durante cinco minutos. Después de cinco minutos, la cantidad restante de la tercera premezcla se
5 añadió durante 45 minutos. La temperatura se dejó aumentar sin calor externo aplicado. Durante la adición la temperatura máxima fue de 57 ºC. Después de que la adición se completara la temperatura fue de 51 ºC. El control de temperatura se ajustó a 52 ºC. La tercera premezcla se aclaró con 108,4 partes de agua desionizada y se añadió al lote. El lote se mantuvo durante 1,5 horas y se enfrío después. Este proporcionó una emulsión al 33,1 % en sólidos, índice de acidez de 27,1, pH de 7,9, y una viscosidad de 12 s (Copa Ford Número 4).
10 Etapa D
Se añadieron a 1473,75 partes de la emulsión de la Etapa C, 26,25 partes de DMEOA para aumentar el pH a 8,6. Usando 1330,18 partes de este material de pH aumentado, se añadieron 89,51 partes de etilenglicol, 16,65 partes
15 de éster dibásico, 16,67 partes de DOWANOL PM, 5,17 partes de xileno, 17,5 partes de una solución de sólidos al 50 % de un fenólico fenol-formaldehído, y 24,57 partes de MICHEM 160 PFE. Se determinó esta formulación para que tuviera sólidos al 30,1 %, viscosidad Ford Número 4 de 12 segundos y 1,05 kg/l (8,75 libras por galón).
La composición de la Etapa D se aplicó a paneles de aluminio sin cromo y se secó en horno durante 10 segundos
20 para conseguir un pico de temperatura de metal de 215 ºC (420 ºF). Un segundo conjunto se secó en horno durante 10 segundos para conseguir un pico de temperatura de metal de 227 ºC (440 ºF). Los resultados del ensayo de la tapa de bebida de este ejemplo, frente a unas fórmulas de control basadas en agua y basadas en disolvente comerciales, se muestran en las Tablas 26 y 27.
- Tabla 26
- Ensayo Comparativo de Curado del Ejemplo 9 Etapa D a 215 ºC (420 ºF)
- Control basado en Agua1
- Control basado en Disolvente2 Ejemplo 9 Etapa D
- MEK
- 44 34 38
- Biselado3
- 0,0457 0,0457 0,000
- COF
- 0,061 0,066 0,063
- Pasteurización4
- Alteración superficial del color
- 10 10 8 a 96
- Adhesión
- 10 10 10
- Retorta de Agua5
- Alteración superficial del color
- 10 10 4 a 106
- Adhesión
- 10 10
- Continuidad de Tapa
- Inicial Después Inicial Después Inicial Después
- Pasteurización
- 0,08 0,12 0,0 0,30 0,0 0,5
- Retorta de Agua
- 0,10 0,4 0,02 0,72 0,27 1,2
- 1 Recubrimiento de tapa de bebida disponible comercialmente de Valspar código 13Q80AG. 2 Recubrimiento de tapa de bebida disponible comercialmente de Valspar código 92X205S. 3 Realizado después de una pasteurización de 45 minutos a 85 ºC (185 ºF). Medido en centímetros (cm). 4 30 minutos a 85 ºC (185 ºF). 5 90 minutos a 121 ºC (250 ºF). 6 Alteración superficial del color inicial observada que mejora dentro de 5 minutos.
39
- Tabla 27
- Ensayo Comparativo de Curado del Ejemplo 9 Etapa D a 227 ºC (440 ºF)
- Control basado en Agua1
- Control basado en Disolvente2 Ejemplo 9 Etapa D
- MEK
- 52 37 40
- Biselado3
- 0,0559 0,0356 0,000
- COF
- 0,059 0,065 0,063
- Pasteurización4
- Alteración superficial del color
- 10 10 8 a 106
- Adhesión
- 10 10 10
- Retorta de Agua5
- Alteración superficial del color
- 10 10 6 a 106
- Adhesión
- 10 10
- Continuidad de Tapa
- Inicial Después Inicial Después Inicial Después
- Pasteurización
- 0,0 0,48 0,07 0,23 0,1 0,8
- Retorta de Agua
- 0,05 0,4 0,25 1,5 0,35 0,8
- 1 Recubrimiento de tapa de bebida disponible comercialmente de Valspar código 13Q80AG. 2 Recubrimiento de tapa de bebida disponible comercialmente de Valspar código 92X205S. 3 Realizado después de una pasteurización de 45 minutos a 85 ºC (185 ºF). Medido en cm. 4 30 minutos a 85 ºC (185 ºF). 5 90 minutos a 121 ºC (250 ºF). 6 Alteración superficial del color inicial observada que mejora dentro de 5 minutos.
Ejemplo 10
5 El Ejemplo 10 ilustra el uso de una sal de polímero ácido-funcional diferente como estabilizador para una emulsión de la presente invención.
Etapa 1
10 Se colocan aproximadamente 1055 partes de BPA en un matraz junto con aproximadamente 1684 partes de resina epoxi líquida (EPON 828), 85 partes de metil isobutil cetona, y de 2 a 3 partes de Catalyst 1201. La temperatura se ajusta a 160 ºC y los contenidos se calientan después durante aproximadamente tres horas para conseguir un valor epoxi del material de aproximadamente 0,003. El lote se ajusta después para que tenga 2684,2 partes de este
15 material en el matraz. Añadido al matraz hay 145,0 partes de metil isobutil cetona y 294,7 partes de anhídrido succínico. La temperatura se mantiene a 120-135 ºC durante dos horas. Después de mantener dos horas, se añaden 124,8 partes de agua desionizada y una premezcla de 214,2 partes de DMEA con 265,8 partes de agua desionizada. Después, se añaden 6325,8 partes de agua desionizada. El material se enfría, y debería dar como resultado un producto con valores objetivo de sólidos del 26 % al 27 %, un índice de acidez de aproximadamente 72,
20 un pH de aproximadamente 7 a 9, y una viscosidad Ford Número 4 de 15 Segundos. Este material se usa en la Etapa 2.
Etapa 2
25 Se equipa un matraz de 5 litros con un agitador, condensador de reflujo, termopar, manta calefactora, y una atmósfera protectora de nitrógeno. En el matraz se añaden aproximadamente 1183 partes del material de la Etapa 1 y 780 partes de agua desionizada. Se prepara una premezcla de 7,25 partes de ácido eritórbico, 6,5 partes de DMEA, y 77 partes de agua desionizada. Esta premezcla inicial y 0,18 partes de HAMP-OL 4,5 % Iron se añaden al matraz. Los contenidos del matraz se calientan a 30 ºC. En un recipiente separado se prepara una premezcla de
30 monómero de 249 partes de estireno, 114 de BA, 107 partes de BMA, 178 partes de HEMA, 36 partes de IBMA, y 28 partes de GMA. Se prepara una tercera premezcla de 7,25 partes de TRIGONOX A-W70 y 82,2 partes de agua desionizada. Una vez que se han preparado todas las premezclas y el matraz está a 30 ºC, se ajusta el agitador a 240 rpm y se añade toda la premezcla de monómero. El recipiente de premezcla de monómero se aclara con 82
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